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February 2008.
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Applied Petrography Group, February 2008.
Contents
Foreword
1. Aims
2. Equipment
3. Sampling
4. Macroscopic analysis
6. Petrographic analysis
7. Quantification
8. Reporting
10. References
11. Definitions
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Foreword
Lime binders in mortar and concrete were replaced progressively by cement during
the 19th Century and since the early 20th Century have been uncommon in UK
building materials. As a result many petrographers who are experienced in the
petrographic examination of concrete might not be aware of issues relevant to the
analysis of lime-based materials.
The terms mortar, plaster and render commonly refer to binder / aggregate mixes
produced for a range of building purposes. In the following sections of this document,
the word mortar is used to describe a binder / aggregate mixture regardless of origin
or function.
Sections in the Code of Practice that cover sample investigation contain a listing of
which features should be examined at each stage of analysis and a discussion of some
of the problematic issues associated with investigation of mortars and other similar
materials.
This Code of Practice is one of three being drafted by the Applied Petrography Group.
The other two cover the petrographic examination of cement based materials and
aggregates.
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1. AIMS
This Code of Practice describes methods for the microscopical examination of lime
based mortars, renders, plasters and other building materials. Suggested procedures
are given for the preparation of thin sections and for the techniques of examining thin
sections with the petrological microscope. In many cases the equipment used and
preparation techniques are similar to those used in examination of samples of
concrete. Some aspects of sampling and examination, however, require additional
information to ensure that the analysis is of maximum benefit.
2 EQUIPMENT
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• Plate glass sheet to be used for final hand finishing of thin sections using an
oil / carborundum abrasive slurry.
• Polishing machines with felt pads for use with abrasive diamond pastes for
polishing to a mirror finish suitable for reflected light examination and for
quantitative SEM microanalysis.
2.1.4 Ovens
For drying of samples prior to preparation a temperature of 70 oC ± 5oC (or 40oC if the
binder contains gypsum) is recommended. Elevated temperatures of curing are
required for some types of epoxy resin. The curing of such resins should be carried
out at temperatures not exceeding 45oC. Ovens of this type are also suitable for drying
specimens prior to their vacuum impregnation with epoxy resin.
2.1.6 Consumables
Common materials used in the UK for the preparation of thin sections would include
the following:
• Low viscosity epoxy resin for vacuum impregnation of samples. Some cure
exothermically and need to be kept cool during curing if used in large
volumes. Some need slightly elevated temperatures (no more than 45oC to
cure.
• Fluorescent dye that can be dissolved in epoxy resin. Note these are not
commonly used in Petrographic examination of mortars, etc.
• Coloured dyes that can be dissolved in epoxy resin.
• Solvents for cleaning purposes such as petroleum spirit, acetone and
methylated spirits.
• Coolant other than water such as cutting oil.
• UV-Curing adhesive for mounting and covering of thin sections.
• Carborundum abrasive of various grades. One of the most commonly used
grades would be 600-grade.
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3. SAMPLING
Diamond core drilling, or samples taken in lump form are both appropriate. It should
be noted, however, that in the case of historic construction the heterogeneity of the
material can be far greater than that of modern buildings. Great care should, therefore,
be taken in selecting a sample or samples for analysis. Sampling should as far as
possible follow the methods described in section 3 of the APG Code of Practice for
Petrographic Examination of Concrete, BS 4551: Part 2, or other appropriate standard.
Ideally, there should be discussion with professionals to determine the reasons for
sampling and the information required. Such issues are covered in Building Research
Establishment (BRE 1995), Ellis (2002), English Heritage (1988) and Historic
Scotland (1995 & 2007).
During the site visit as much information as possible should be gained regarding the
sample and its context within the building. The function of the sample in the structure,
the type of mortar (pointing, plaster, render, etc.) and the condition of the material
should be described. Other data of value include (where relevant):
The age of the sample, if known, along with any historical information relating to the
building / structure, or specific area, such as exposure to fire, blast damage, etc., will
all aid the petrographer in the interpretation of their observations. If sampled by a
third party, photographs of the structure and the sample location will also be of value.
Sample size is difficult to specify and there might be constraints of how much
material may be removed through building type or considerations of conservation
aesthetics. As historic mortars can contain coarse-grained aggregate and quantities of
unmixed binder larger samples than those commonly obtained through diamond core
drilling might be required. An important point to emphasise if samples are to be taken
by a third party is that samples comprising powder (sampled by abrasion causing
disaggregation of the mortar) are of limited use. It is often advisable to obtain more
than one sample to ensure that the report will be applicable to the materials in the
building / structure under investigation. This is of particular importance if the
structure has been extended, modified or repaired.
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Selection of a sub-sample for thin sectioning is also dependant in part on the reasons
for analysis. Commonly a sample will be analysed with the intention of examining the
mortar / air or mortar / stone interface, in which case the thin section will be cut
perpendicular to this interface. It is therefore recommended that samples include a
part of the adjoining masonry material (stone or brick in the case of bedding and
jointing mortars), and cross-layer interfaces (in the case of plasters, renders and
pointing mortars).
In examining older mortars it is of value to take note of the geology in the area that
the building / structure is situated, or, if known, the source of the lime. There are few
limestone sources in the north of the UK that produced pure, high calcium limes.
Many limestones in the UK contain a proportion of dolomite.
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4. MACROSCOPIC ANALYSIS
During examination of the hand specimen all samples should be described in terms of:
4.1.2 Any evidence for damage or degradation to the sample including surfaces and
interfaces
4.1.5 Condition of the binder (paste) including the presence of relict limestone and
relict fuel
4.2 Discussion
The function of the sample should be described with respect to the observations made
in section 3. This is best determined in macroscopic analysis as a thin section might
provide no information on sample origins.
In wall coverings the number of coats and the thickness of each coat should be
measured and the bond at each interface assessed. The presence of admixtures or
additives should be noted and a visual estimate of the proportions made. If hair, straw
or other fibres are present then their distribution throughout the mortar should be
noted along with their orientation relative to any interfaces. A description of the
condition of such fibres e.g. brittle, denatured, replaced by calcite or gypsum can also
be of value.
In lime based materials the amount of carbonation can be examined using a solution
of Phenolphthalein1 (Vogel, 1948). This reacts with calcium hydroxide to give a
strong pink colouration. This is commonly of use in modern materials but
uncarbonated calcium hydroxide has been found in dense mortars in excess of 100
years old. An assessment of carbonation should only be made using a freshly exposed,
clean surface or an uncovered thin section as contamination from other building
materials is a common problem.
The hydraulicity of the binder (i.e. the amount of chemical set) is best assessed by a
combination of hand specimen and thin section examination (ASTM C25-06, Crisci et
al., 2004). There might not always appear to be a clear relationship between binder
microstructure and hydraulic content, but this is dependant on the sample condition.
1
A solution comprising 1g phenolphthalein, 100ml of ethyl alcohol and 100ml water.
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Additional analysis, such as by XRD XRF and SEM or quantification of soluble silica
content, might assist in clarifying situations where doubt exists.
The use of polished surface examination is more common in the analysis of concrete
and the method is described in sections 4.1 and 5.3 of the Code of Practice for
Petrographic Examination of Concrete.
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5.1 Introduction
This section provides a description of a possible method for thin section preparation.
This method of preparation is commonly employed in the UK, however it should be
noted that many other procedures and types of equipment are available. For all
methods employed it is essential that the following precautions be taken:
In most cases it is possible to carry out initial cutting using a water-lubricated large
diameter diamond saw. In the case of very weak or friable samples, such those
affected by fire damage or acid attack, it is essential that the sample surface be
vacuum impregnated with resin in order to consolidate the surfaces prior to any
cutting being carried out.
It is desirable that the final states of cutting be carried out using a precision small-
diameter saw in order to minimise the amount of damage in the cut surface that needs
to be removed prior to mounting on to glass microscope slide.
5.3 Impregnation
In order to produce high quality polished surfaces – particularly if the sample is very
porous – it is essential that the sample be vacuum impregnated with a low viscosity
epoxy resin prior to polishing and grinding. The use of a coloured dye is
recommended in order to assist in the determination of porosity and microcracking.
Fluorescent dyes may also be employed for this purpose. The most effective means of
impregnation is to place the sample in a vacuum chamber and evacuate prior to the
introduction of the impregnating resin.
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adhesive. It is important in mounting the specimen on to the glass that the thickness of
the bond is of a controlled thickness and is kept to a minimum under the specimen.
Once bonded on to glass the specimen is then ready for the excess material to be cut
off. This is done using a precision, oil lubricated diamond saw and when complete
should leave a section thickness of the order of 1mm.
The thin sample is then ground down in stages to a thickness of approximately 150 to
200 µm using diamond surface-grinding equipment lubricated by oil. Further lapping
using a precision vacuum chuck is used to take the section to a thickness of about
40µm if it is to be hand finished. With some types of equipment it is possible to take
the thin section down to its final thickness using very fine diamond grinding wheels.
Using a petrological microscope to measure the thickness of the thin section the
section can be hand finished down to its final thickness of 25 – 30 µm. The
birefringence of quartz particles present in the aggregate commonly provides a
convenient way of judging the thickness of the thin section during hand finishing.
5.9 Covering
It is important that on completion the final section be thoroughly cleaned and then
covered using a glass cover slip. This is to prevent damage to the sample after its
preparation and is also important to reduce light scattering during the examination of
the thin section.
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6. PETROGRAPHIC ANALYSIS
6.1.1 Details of the minerals and rock types present within the aggregate
6.1.4 Details of the type, condition, crystallinity, and if present degradation of the
binder
6.2 Discussion
At least one thin section and preferably more depending on the specific objectives of
the investigation should be prepared for each sample as appropriate and each thin
section should measure ideally 45 x 70 mm. The location and number of thin sections
required should be decided by the petrographer during the preliminary macroscopic
examination of the samples. However it is often advantageous that at least one section
be made from a plate cut at right angles to the external surface of the sample, so that
the outer ~70 mm are included in the section. Pore geometry should be noted as there
is some evidence that pore shape evolves over time.
The heterogeneity of historic building materials is such that quantitative analysis (i.e.
point counting) should be used only if considered essential to the examination (ASTM
C457, Leslie & Gibbons, 2000).
Binders made using gypsum (calcium sulphate hydrate) or a mixture of gypsum and
calcite are difficult to identify in thin section unless there is recrystallisation of coarse
crystalline gypsum within binder cavities. Gypsum rich binders are relatively easy to
identify in hand specimen. If there is a need to identify microcrystalline gypsum
within a binder then a stain using mercuric nitrate can be used.
Binders with a clay component (i.e. where unburned clay was used either exclusively
as the binder material or mixed with lime) require the application of additional
analysis techniques. The mineralogy can be determined by employing XRD analysis
and this is often assisted by the examination of recovered residue following a simple
acid dissolution of any lime binder component.
The use of organic additives in lime based binders cannot be identified in thin section.
However it is not uncommon to distinguish the effects of the presence of organic
components in the mortar. Simple spot tests using oxidising agents and the textural
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appearance in thin section might highlight the presence of organic material but
identification of the form of the component present will require the use of complex
analyis. It must also be born in mind that organic materials are prone to degradation
and the residual components detected may not be representative of those added.
Care should be taken to identify areas of binder where there has been either
dissolution or re-precipitation of calcium carbonate. The mobilisation of calcium
carbonate binder is a common occurrence in lime-based materials and can cause a
significant change in the bulk chemical composition of the sample (Leslie & Hughes,
2002). If this is not identified then there is a risk of significant error in the reporting of
mortar composition. This mobilisation cannot be identified through wet chemical
analysis and petrographic analysis is required to ascertain the dissolution and
reprecipitation of binder.
These comments are equally applicable to dolomitic and gypsipherous binders. Where
reprecipitation occurs, caution should be exercised not to misinterpret the result of
chemical attack such as those produced by externally derived sulphates.
The mortar aggregate analysis should be carried out in accordance with BS 812:103
and the APG Code of Practice for the petrographic examination of aggregate.
Other materials in a mortar might include additions of fibres such as hair (particularly
common in internal plaster work, brick dust or other pozzolanic materials (Gibbons,
1997) and impurities from the kiln in the form of relict fuel and relict limestone
(either under burnt or over burnt) might also be present (Leslie & Hughes, 2005).
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7. QUANTIFICATION
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8. REPORTING
A report should include the following information. It is recommended that the data are
recorded in table form as shown in section 9 of this document.
• If appropriate, comment may be given on the age of the sample, its response to
exposure / weathering, etc, and if required guidance given on its conservation,
replication or the design of a compatible restoration mortar.
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Laboratory ref.
Sample ref.
Sample preparation
details
Sample dimensions:
Core diameter (mm)
Core length (mm)
Number of pieces
Description of outer
surface
Description of inner
surfaces and other
interfaces
Binder colour
Binder texture
Lime inclusions:
Size
Proportion of binder
Coarse cracking:
(>0.1 mm wide)
Fine cracking:
(0.01-0.10 mm)
Carbonation:
Typical depth (mm)
Coarse aggregate
distribution:
Measured / estimated
porosity (voids)
(Vol. %)
Supplementary notes:
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Laboratory ref.
Sample ref.
Coarse aggregate:
Maximum size (mm)
Typical shape
Major rock / mineral
types
Minor rock / mineral
types
Trace rock / mineral
types
Fine aggregate:
Grading
(estimated BS 882 (fine-
medium-coarse) grading
classification)
Maximum size (mm)
Typical shape
Major rock / mineral
types
Minor rock / mineral
types
Trace rock / mineral
types
Evidence for
aggregate reactions
(e.g. alkali reaction, unstable
slag, pyrite)
Aggregate surface
details
(include evidence for
aggregate shrinkage, DEF or
AAR)
Artificial aggregate
(e.g. brick, slag, clinker)
Other material
(e.g. hair, straw)
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Laboratory ref.
Sample ref.
Binder type
Binder texture
(details of porosity, grain size)
Portlandite
(approx. vol.% of binder)
Lime inclusions
Size
Texture
Vol. % of binder
Porosity (voids)
General vol. %
Porosity distribution
Micro cracking
Void fillings and
abundance
Laboratory ref.
Sample ref.
VOLUME PROPORTIONS:
Binder (set) %
Fine aggregate %
Coarse aggregate %
Porosity (voids) %
Form in which binder was
mixed (if known)
Binder constituents
WEIGHT PROPORTIONS:
Fine aggregate (kg/m3)
Coarse aggregate (kg/m3)
Binder (unset)1 (kg/m3)
Water (kg/m3)
Aggregate / binder ratio
Binder content
(Wt. %)2
1 Note different and approximate densities of lime binder in the form of putty
(!1350 kg/m3) dry hydrate (1000 kg/m3) and quicklime (<900 kg/m3).
2 Calculated on an equivalent oven dried basis.
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10. REFERENCES
ASTM C1324-05 Standard Test Method for Examination and Analysis of Hardened
Masonry Mortar
BS 4551: Part 2 Methods of testing mortars, screeds and plasters. Chemical analysis
and aggregate grading
BS 6463 : 103 Quicklime, hydrated lime and natural calcium carbonate. Methods for
physical testing
Crisci, G.M., Franzini, M., Lezzerini, M., Mannoni, T & Riccardi, M.P. 2004
Ancient mortars and their binder. Periodico di Mineralogica, Vol. 73, 259-268.
English Heritage 1988 Practical Building Conservation (v.3): Mortars, Plasters and
Renders. English Heritage Technical Handbook.
Historic Scotland 1995 Preparation and use of lime mortars, second edition.
Historic Scotland Technical Advice Note 1.
Historic Scotland 2007 The use of lime & cement in traditional buildings.
Information for Historic Building Owners.
Leslie, A.B. & Gibbons, P. 2000 Mortar analysis and repair specification in the
conservation of Scottish historic buildings. In Bartos, P., Groot, C. & Hughes, J
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Leslie, A.B. & Hughes, J.J. 2002 Binder microstructure in lime mortars: implications
for the interpretation of analysis results. Quarterly Journal of Engineering Geology
and Hydrogeology, 35, 257 – 263.
Leslie, A.B. & Hughes, J.J. 2005 High temperature slag formation in historic
Scottish mortars: Evidence for production dynamics in 18th - 19th Century lime
production from Charlestown. In: Materials Characterisation, 53, 181-186.
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11. DEFINITIONS2
In addition to those given below further definitions are given in the codes of practice
covering cements and aggregates.
Aggregate Any material which, when combined with a binder, forms a mortar.
This can include sand, crushed rock, brick dust or other mineral fillers.
Builders lime Non hydraulic, powdered dry hydrate lime, available in building
suppliers.
• Macrocrack: These are cracks that are readily visible to the naked eye without
the aid of a stereo binocular microscope and are typically >0.10 mm wide.
• Macroscopic cracks: These cracks are visible in the hand specimen or with the
aid of a stereo binocular microscope and are typically >0.01 mm wide.
• Fine crack: These are cracks that are only readily visible with a stereo
binocular microscope or in thin section. Cracks of this type are typically
between 0.01 and 0.10 mm wide.
• Microcracking: These cracks cannot be detected with a stereo binocular
microscope. They are typically <0.01 mm wide and are most easily seen in
petrographic thin sections containing stained or fluorescent resins.
Dolomitic lime Lime derived from dolomite (mainly consisting of calcium and
magnesium oxide, typically 35 to 45% by weight magnesium carbonate).
Dry hydrate A binder in which calcium oxide (quicklime) has been hydrated with
sufficient water to form calcium hydroxide in the form of a dry powder.
2
See also the Glossary of Terms in the Code of Practice for the Petrographic Examination of Building
Materials produced by the APG.
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Hardburned lime Quicklime that has been exposed to prolonged calcination and
that might be poorly reactive as a result. Also known as over burnt lime.
Hydrated lime Lime that has been hydrated either with sufficient water to form
calcium hydroxide in the form of a powder or with excess water to form a putty.
Hydraulic lime Impure lime containing clays or other materials that give a
mortar a chemical set that is commonly quicker than the carbonation of pure, non-
hydraulic lime. The strength of the chemical set can depend on the quantity of clays,
etc., but also on the conditions of manufacture. Natural cement is a particularly strong
variant of a hydraulic lime. Hydraulic limes cannot be stored in the form of putty as in
the aqueous environment the chemical set will take place.
Lime putty A form of non-hydraulic lime in which calcium oxide (quicklime) has
been hydrated with excess water to form soft, workable putty.
Macroscopic This is a general term referring to features that are visible to the naked
eye or with the aid of a stereo microscope.
Magnesian lime Lime derived from calcite containing more than 5% by weight
of magnesium oxide (typically 5 to 35%).
Mortar A general term for a binder / aggregate mix used in construction. More
specifically the term mortar refers to a mix used to bed masonry blocks (pointing) or
to fill a cavity between two masonry leaves (wall core). Aggregate can vary in grain
size from a fine powder (<0.1 mm) filling 1-2 mm joints between ashlar masonry to
coarse gravel (>50 mm) in wall core.
Natural cement Natural cements are hydraulic cements produced by mining and
burning deposits of limestone and clay with a specific chemical composition within a
narrow range. Strength and uniformity of natural cements are lower than for Portland
cements. Natural cements were common in 19th and early 20th century construction
until superseded by Portland cement.
Portland cement Portland cement is the most common form of binder used in
concrete and is manufactured from the burning of limestone and an alumino-silicate
rock (clay or shale) at temperatures of up to 1500oC. There are many forms of
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